CN103666419B - A kind of oil well cement composite organic defoamer - Google Patents
A kind of oil well cement composite organic defoamer Download PDFInfo
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- CN103666419B CN103666419B CN201310652483.9A CN201310652483A CN103666419B CN 103666419 B CN103666419 B CN 103666419B CN 201310652483 A CN201310652483 A CN 201310652483A CN 103666419 B CN103666419 B CN 103666419B
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- defoamer
- emulsifying agent
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/46—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
- C09K8/467—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement containing additives for specific purposes
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/40—Compounds containing silicon, titanium or zirconium or other organo-metallic compounds; Organo-clays; Organo-inorganic complexes
- C04B24/42—Organo-silicon compounds
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/50—Defoamers, air detrainers
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Structural Engineering (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a kind of oil well cement efficient composite organic silicon defoamer and preparation method thereof, puddle the froth breaking in process for the cementing slurry high speed shear containing multiple admixture, press down bubble.Be calculated in mass percent, the raw material of preparation has 10%-20% polydimethylsiloxane, 2%-4% white carbon black, 5%-10% tributyl phosphate, 5%-7% compound emulsifying agent, 1%-2% stablizer, and surplus is water.Preparation method: add polydimethylsiloxane, white carbon black successively in reactor, be warming up to 110-150 DEG C, stir with 65 revs/min of-80 revs/min of speed and make the abundant homogenizing of two materials, reaction 1.5-2.5 hour, be cooled to 70-80 DEG C, add tributyl phosphate and emulsifying agent, stirring reaction 15-18 minute, stablizer is soluble in water, the water being dissolved with stablizer is added in reactor, continue constant temperature and stir 1.5-2 hour, stir bottom discharge, obtain product.Defoamer of the present invention is with low cost compared to common silicone based defoamer, manufacture craft simple, has froth breaking concurrently, presses down bubble function, do not affect grout multiviscosisty performance, can significantly improve its rheological and Behavior of Hardened Cement Paste ultimate compression strength.
Description
Technical field
The present invention relates to a kind of efficient composite organic silicon defoamer, be specially adapted to froth breaking, the oil well cement efficient composite organic silicon defoamer pressing down bubble and preparation method thereof in the oil well cement paste preparation of oil well cementing working-yard.
Background technology
In reinforcing oil well construction operation process, in order to the API standard cement kind enabling working-yard limited meets the cementing conditions emerged in an endless stream, multiple admixture must be added to improve the over-all properties of grout in oil well cement paste, but the oil well cement paste being added with admixture can produce a large amount of bubble under high velocity agitation, this bubble has higher glutinousness, easily be stranded in slurry inside, common defoamer is difficult to eliminate.Under sequential production condition, as can not froth breaking fast, grout actual density will be made to be significantly less than actual value, cause cement strength and consolidation strength to reduce, meanwhile, due to this error message by Real-time Feedback to stock mixing system, the ratio of oil well cement and water with slurry will be caused to change, also have impact on the effective content of various admixture in grout simultaneously, cause the parameter such as its rheological property, fluid loss, thickening time to produce deviation with design, time serious, directly cause cementing operation failure.Therefore, a kind of defoamer of excellent property occupies very important status in cementing operation.
And it is current special very few for preparation method's studies in China of the defoamer of well cementing mortar architecture, and existing domestic defoamer can not meet the needs of drilling technology, not only defoaming effect is poor, and product category is also very few, can not adapt to various different oil well cement slurry system and application conditions.The oil well cement paste defoamer of excellent property is except requiring to have except higher defoaming capacity, also require that to mortar architecture be inertia, not with other admixture react with, be applicable to fresh water, salty mud system, do not affect grout multiviscosisty performance, ultimate compression strength, rheological property etc.In prior art, the basic preparation technology of defoamer is similar, and difference selects for different application purposes or prepared different froth breaking materials, have employed different formulas and concrete compound emulsion technique.
Summary of the invention
Object of the present invention is just to provide a kind of oil well cement efficient composite organic silicon defoamer and preparation method thereof, and the cementing slurry high speed shear be exclusively used in containing multiple admixture is puddled froth breaking in process, pressed down bubble.Defoamer of the present invention is with low cost compared to common silicone based defoamer, manufacture craft simple, has froth breaking concurrently, presses down bubble function, do not affect grout multiviscosisty performance, can significantly improve its rheological and Behavior of Hardened Cement Paste ultimate compression strength.
Object of the present invention realizes by following measures: a kind of oil well cement efficient composite organic silicon defoamer, be calculated in mass percent, the raw material of preparation has 10%-20% polydimethylsiloxane, 2%-4% white carbon black, 5%-10% tributyl phosphate, 5%-7% compound emulsifying agent, 1%-2% stablizer, and surplus is water.
Described compound emulsifying agent is span and tween class mixture, the theoretical HLB value 8.0-9.0 of emulsifying agent after mixing.
Described compound emulsifying agent is the mixture of this dish-60, Span-80 and Tween-60.
In mass ratio, the blending ratio of described this dish-60, Tween-60 and Span-80 is 1.3-1.97:2.0:1.3-1.97.
Described stablizer is organobentonite.
The preparation method of above-mentioned oil well cement efficient composite organic silicon defoamer, comprise the following steps: in reactor, add polydimethylsiloxane, white carbon black successively, be warming up to 110-150 DEG C, stir with 65 revs/min of-80 revs/min of speed and make the abundant homogenizing of two materials, reaction 1.5-2.5 hour, be cooled to 70-80 DEG C, add tributyl phosphate and compound emulsifying agent, stirring reaction 15-18 minute, stablizer is soluble in water, adds in reactor by the water being dissolved with stablizer, continues constant temperature and stirs 1.5-2 hour, stir bottom discharge, obtain product.
The present invention has following advantage:
(1) be specifically designed to oil well cement paste process for preparation, froth breaking, to press down bubble ability strong, and bentonite adds makes its stability stronger.
(2) be inertia to mortar architecture, not with other admixture react with, be applicable to fresh water, salty mud system, do not affect grout multiviscosisty performance, significantly improve ultimate compression strength and the rheological property of Behavior of Hardened Cement Paste.
(3) preparation method is simple, reaction conditions is gentle, with low cost, is easy to realize.
Accompanying drawing explanation
Fig. 1 is that defoamer addition of the present invention is on the impact of cement slurry density recovery rate.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail:
Oil well cement efficient composite organic silicon defoamer of the present invention, be calculated in mass percent, the raw material of preparation has 10%-20% polydimethylsiloxane, 2%-4% white carbon black, 5%-10% tributyl phosphate, 5%-7% compound emulsifying agent, 1%-2% stablizer, and surplus is water.
Described compound emulsifying agent is span and tween class mixture, the theoretical HLB value 8.0-9.0 of emulsifying agent after mixing.
Described compound emulsifying agent is the mixture of this dish-60, Span-80 and Tween-60.
In mass ratio, the blending ratio of described this dish-60, Tween-60 and Span-80 is 1.3-1.97:2.0:1.3-1.97.
Described stablizer is organobentonite.
The preparation method of above-mentioned oil well cement efficient composite organic silicon defoamer, comprise the following steps: in reactor, add polydimethylsiloxane, white carbon black successively, be warming up to 110-150 DEG C, stir with 65 revs/min of-80 revs/min of speed and make the abundant homogenizing of two materials, reaction 1.5-2.5 hour, be cooled to 70-80 DEG C, add tributyl phosphate and compound emulsifying agent, stirring reaction 15-18 minute, stablizer is soluble in water, adds in reactor by the water being dissolved with stablizer, continues constant temperature and stirs 1.5-2 hour, stir bottom discharge, obtain product.
It should be noted that: this dish-60 is Sorbitan acid monostearate, Span-80 is sorbitan monooleate, Tween-60 is polyoxyethylene sorbitan acid monostearate.
The main body froth breaking composition of efficient composite organic silicon defoamer of the present invention is polydimethylsiloxane, and antifoam additives composition is white carbon black, compositely reduces costs with tributyl phosphate, improves defoaming effectiveness further.
If the consumption of polydimethylsiloxane is less than 10% massfraction in system, then can not realizes good froth breaking effect, defoamer dosage can be strengthened, if higher than 20% massfraction, defoaming effectiveness can not be improved and also can increase cost; If white carbon black consumption is less than 2% massfraction or higher than 4% massfraction, all will extends foam time, and consumption too much can make aqueous emulsion of dimethyl polysiloxane fluid stability reduce; If tributyl phosphate consumption is less than 5% massfraction, defoaming effectiveness improves not obvious, if higher than 10% massfraction, its defoaming effectiveness also can not increase thereupon; If compound emulsifying agent adds up to consumption to be less than 5% massfraction, Emulsion consistencies is little, dewatering ability is poor, if higher than 7% massfraction, then defoaming effect is relatively low.
Meanwhile, in order to make defoamer emulsion obtain the stable of long period, also add organobentonite as stablizer, have stability, thickening property, consumption is between 1%-2%, and its consumption is too low, and stability of emulsion is poor, and consumption is too high, and emulsion viscosity is excessive.Adding water is to make its emulsification, and product is white uniformity emulsion.
Set forth the present invention with specific embodiment below, but embodiment is not limited to its scope.
Embodiment 1
Raw material is prepared with massfraction
Formula (1)
Get 10% polydimethylsiloxane, 2% white carbon black, 5% tributyl phosphate, 1.43% this dish-60,2.2% Tween-60,1.43% Span-80,1% organobentonite, surplus is water.
Formula (2)
Get 15% polydimethylsiloxane, 3% white carbon black, 8% tributyl phosphate, 1.7% this dish-60,2.5% Tween-60,1.7% Span-80,1.5% organobentonite, surplus is water.
Formula (3)
Get 20% polydimethylsiloxane, 4% white carbon black, 10% tributyl phosphate, 2.1% this dish-60,2.8% Tween-60,2.1% Span-80,2% organobentonite, surplus is water.
Preparation method: select formula (1) or (2) or (3) wherein a group, polydimethylsiloxane, white carbon black is added successively in reactor, be warming up to 110-150 DEG C, stir with 80 revs/min of speed and make the abundant homogenizing of two materials, reaction 1.5-2.5 hour, be cooled to 70-80 DEG C, add tributyl phosphate and compound emulsifying agent, stirring reaction 15-18 minute, organobentonite is soluble in water, will be dissolved with bentonite water and add in reactor, continues constant temperature and stirs 1.5-2 hour, stir bottom discharge, obtain white " milky " liquid product.
Anti-foam product of the present invention is up to state standards the requirement of GB/T26527-2011 silicone antifoam agent.Experiment Raw composition all derives from commercially available.
Embodiment 2
Product performance are evaluated
(1) stability
Get a certain amount of dilution of defoamer sample of the present invention 5 times, with the centrifugal 20min of 3500r/min rotating speed on supercentrifuge, observe its outward appearance without layering.
(2) froth breaking and suds suppressing properties
Measure in letter at 600mL, add the Sodium dodecylbenzene sulfonate expanding foam solution that 100mL concentration is 1.5%, start recycle pump bubbling and reach 500mL to lather volume, add a certain amount of defoamer of the present invention, start timing, record foam time of all eliminating, and then record lather volume and reach 500mL required time again, press down the bubble time for defoamer of the present invention.The results are shown in Table 1.
Table 1 defoamer of the present invention with abroad with defoamer froth breaking and press down the bubble time and contrast
| Experimental group | Foam time/s | Press down bubble time/s |
| Embodiment 1 fills a prescription (1) | 20 | 57 |
| Embodiment 1 fills a prescription (2) | 18 | 54 |
| Embodiment 1 fills a prescription (3) | 23 | 55 |
| The same defoamer of certain import | 21 | 55 |
Note: keep constant temperature 25 DEG C in test, pH is 7.
Result: as shown in Table 1, froth breaking, the suds suppressing properties of defoamer of the present invention are suitable with import like product, superior performance.
Embodiment 3
Defoamer of the present invention is to the evaluation of oil well cement paste antifoam performance
The method required according to National Standard of the People's Republic of China GB/T19139-2003 " oil-well cement test method " chapter 5 prepares cement paste, Sample FormulationsThe is G class g cement: micro-silicon is 5:1, high temperature water retaining 1.8%, dispersion agent 0.5%, mixing water and cement dry ash mass ratio are 1.0.
(1) defoamer addition is on the impact of oil well cement pulp density recovery rate
Prepare three parts of same oil well cement pastes, first part of grout pressurized liquid density measurement density is 1.63g/cm
3; Stir second part of grout in required time again, measuring its density with liquidensitometer is 1.13g/cm
3; In the 3rd part of grout process for preparation, add the defoamer of the present invention of 0.15%, measuring its density with liquidensitometer after stirring by specific time is 1.6g/cm
3.
Result:
Conclusion: when defoamer addition of the present invention is 0.15%, the defoaming effect in oil well cement paste is desirable, and the density of grout can be made to recover 94.7%, (see Fig. 1).
(2) on the impact of hardened oilwell cement ultimate compression strength
The method steps required according to National Standard of the People's Republic of China GB/T19139-2003 " oil-well cement test method " chapter 7 carries out the Behavior of Hardened Cement Paste compressive strength test containing 0.15% defoamer of the present invention, 80 DEG C of ordinary pressure curing 24h.
Record cement strength: 14.1MPa
(3) on the impact of oil well cement paste multiviscosisty performance
The method steps test required according to National Standard of the People's Republic of China GB/T19139-2003 " oil-well cement test method " chapter 9 containing 0.15% defoamer slurry of the present invention 80 DEG C, 46.5MPa, heating-up time be thickening time under 45min condition, initial consistency, multiviscosisty is linear.
Result: initial consistency 16.2Bc, the thickening time is 168min, and multiviscosisty is normally linear, does not have disadvantageous effect to grout multiviscosisty performance.
(4) on the impact of oil well cement paste rheological property
According to the method steps that National Standard of the People's Republic of China GB/T19139-2003 " oil-well cement test method " chapter 12 requires, the grout containing 0.15% defoamer of the present invention be made into is heated to 85 DEG C of Keep agitation 20min again in normal pressure multiviscosity meter, then pour into scale marks in six fast rotational viscosimeter sample cups immediately, the rheological parameter value of test slurry.
Result: recording Rheological Index n is 0.78, and multiviscosisty COEFFICIENT K is 0.12.
Table 2 defoamer of the present invention is on the impact of oil well cement paste performance
Above-described embodiment is only for illustration of technological thought of the present invention and feature, its object is to enable those skilled in the art understand content of the present invention and implement according to this, only can not limit the scope of the claims of the present invention with the present embodiment, namely the equal change done of all disclosed spirit or modification, still drop in the scope of the claims of the present invention.
Claims (3)
1. an oil well cement composite organic defoamer, it is characterized in that, be calculated in mass percent, the raw material of preparation has 10%-20% polydimethylsiloxane, 2%-4% white carbon black, 5%-10% tributyl phosphate, 5%-7% compound emulsifying agent, 1%-2% stablizer organobentonite, and surplus is water; Described compound emulsifying agent is span and tween class mixture, the theoretical HLB value 8.0-9.0 of emulsifying agent after mixing;
Preparation method comprises the following steps: in reactor, add polydimethylsiloxane, white carbon black successively, be warming up to 110-150 DEG C, stir with 65 revs/min of-80 revs/min of speed and make the abundant homogenizing of two materials, reaction 1.5-2.5 hour, be cooled to 70-80 DEG C, add tributyl phosphate and compound emulsifying agent, stirring reaction 15-18 minute, stablizer is soluble in water, the water being dissolved with stablizer is added in reactor, continue constant temperature and stir 1.5-2 hour, stir bottom discharge, obtain product.
2. oil well cement composite organic defoamer according to claim 1, is characterized in that, described compound emulsifying agent is the mixture of this dish-60, Span-80 and Tween-60.
3. oil well cement composite organic defoamer according to claim 2, is characterized in that, in mass ratio, the blending ratio of described this dish-60, Tween-60 and Span-80 is 1.3-1.97:2.0:1.3-1.97.
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| CN106082775A (en) * | 2016-06-07 | 2016-11-09 | 中国石油集团渤海钻探工程有限公司 | Latex cement defoaming agent and preparation method thereof |
| CN107117851B (en) * | 2017-05-09 | 2019-07-02 | 江苏四新科技应用研究所股份有限公司 | A kind of preparation method of oil-well cement powder defoaming agent |
| CN107177351A (en) * | 2017-06-30 | 2017-09-19 | 四川宏升石油技术开发有限责任公司 | A kind of preparation method of defoamer easy to use |
| CN107200503A (en) * | 2017-06-30 | 2017-09-26 | 四川宏升石油技术开发有限责任公司 | A kind of strong new defoamer of suds ability |
| CN107936939A (en) * | 2017-11-02 | 2018-04-20 | 中国石油集团渤海钻探工程有限公司 | A kind of acidifying foam controller and preparation method thereof |
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| CN108726913B (en) * | 2018-05-28 | 2021-04-27 | 天津中油渤星工程科技有限公司 | Silicon ether composite defoaming agent and preparation method and application thereof |
| CN110156282A (en) * | 2019-05-13 | 2019-08-23 | 深圳申佳原环保科技有限公司 | A kind of shield slurry defoaming agent and preparation method thereof and application method |
| CN112525768A (en) * | 2020-12-25 | 2021-03-19 | 武汉三源特种建材有限责任公司 | Method for detecting defoaming rate of cement base material defoaming agent |
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